 
data_s802
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C28 H20 As I2 N O3 W'
_chemical_formula_weight          931.02
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'As'  'As'   0.0499   2.0058
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)
_symmetry_space_group_name_hall   'P 2ac 2ab'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 
_cell_length_a                    10.5430(3)
_cell_length_b                    16.3150(7)
_cell_length_c                    18.8950(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3250.1(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.23
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.903
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1728
_exptl_absorpt_coefficient_mu     6.490
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             11582
_diffrn_reflns_av_R_equivalents   0.0624
_diffrn_reflns_av_sigmaI/netI     0.2621
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          3.15
_diffrn_reflns_theta_max          25.02
_reflns_number_total              5646
_reflns_number_gt                 3709
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.161(16)
_refine_ls_number_reflns          5646
_refine_ls_number_parameters      296
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0583
_refine_ls_R_factor_gt            0.0438
_refine_ls_wR_factor_ref          0.1433
_refine_ls_wR_factor_gt           0.1246
_refine_ls_goodness_of_fit_ref    0.495
_refine_ls_restrained_S_all       0.495
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
W1 W 0.05164(6) 0.07455(4) 0.98558(3) 0.01896(16) Uani 1 1 d . . .
As1 As -0.15160(14) -0.01831(10) 0.97624(8) 0.0198(3) Uani 1 1 d . . .
I1 I 0.09728(11) -0.03081(7) 1.10279(5) 0.0293(3) Uani 1 1 d . . .
I2 I 0.23445(11) 0.18209(7) 1.04398(6) 0.0323(3) Uani 1 1 d . . .
O1 O 0.0251(11) 0.2369(8) 0.8966(7) 0.037(3) Uani 1 1 d . . .
O2 O 0.3126(12) -0.0047(8) 0.9397(7) 0.039(3) Uani 1 1 d . . .
O3 O 0.0263(13) 0.0196(9) 0.8267(5) 0.043(4) Uani 1 1 d . . .
N1 N -0.0786(14) 0.1379(8) 1.0549(7) 0.029(3) Uani 1 1 d . . .
C1 C -0.2573(17) -0.0636(13) 1.1113(9) 0.039(4) Uani 1 1 d . . .
H1 H -0.1852 -0.0961 1.1153 0.047 Uiso 1 1 calc R . .
C2 C -0.3494(16) -0.0630(13) 1.1660(8) 0.035(4) Uani 1 1 d . . .
H2 H -0.3384 -0.0953 1.2061 0.042 Uiso 1 1 calc R . .
C3 C -0.4593(18) -0.0122(13) 1.1590(9) 0.038(5) Uani 1 1 d . . .
H3 H -0.5218 -0.0124 1.1937 0.046 Uiso 1 1 calc R . .
C4 C -0.4713(19) 0.0373(14) 1.0995(9) 0.043(5) Uani 1 1 d . . .
H4 H -0.5398 0.0729 1.0953 0.052 Uiso 1 1 calc R . .
C5 C -0.3813(15) 0.0334(11) 1.0469(8) 0.028(4) Uani 1 1 d . . .
H5 H -0.3924 0.0650 1.0065 0.033 Uiso 1 1 calc R . .
C6 C -0.2757(14) -0.0155(9) 1.0519(7) 0.018(3) Uani 1 1 d . . .
C7 C -0.0081(17) -0.1606(11) 0.9389(8) 0.031(3) Uani 1 1 d . . .
H7 H 0.0585 -0.1240 0.9324 0.038 Uiso 1 1 calc R . .
C8 C 0.0080(17) -0.2482(11) 0.9266(9) 0.031(3) Uani 1 1 d . . .
H8 H 0.0844 -0.2679 0.9088 0.038 Uiso 1 1 calc R . .
C9 C -0.0874(19) -0.3008(10) 0.9409(8) 0.032(3) Uani 1 1 d . . .
H9 H -0.0738 -0.3568 0.9355 0.039 Uiso 1 1 calc R . .
C10 C -0.1995(18) -0.2748(10) 0.9624(8) 0.032(3) Uani 1 1 d . . .
H10 H -0.2645 -0.3125 0.9693 0.039 Uiso 1 1 calc R . .
C11 C -0.223(2) -0.1890(9) 0.9754(9) 0.035(4) Uani 1 1 d . . .
H11 H -0.3009 -0.1710 0.9928 0.042 Uiso 1 1 calc R . .
C12 C -0.1258(16) -0.1341(10) 0.9607(8) 0.025(2) Uani 1 1 d . . .
C13 C -0.3149(17) -0.0419(12) 0.8555(9) 0.035(3) Uani 1 1 d . . .
H13 H -0.3046 -0.0977 0.8638 0.043 Uiso 1 1 calc R . .
C14 C -0.3952(18) -0.0137(11) 0.7974(9) 0.035(3) Uani 1 1 d . . .
H14 H -0.4361 -0.0514 0.7684 0.043 Uiso 1 1 calc R . .
C15 C -0.4101(18) 0.0701(14) 0.7858(9) 0.042(5) Uani 1 1 d . . .
H15 H -0.4617 0.0894 0.7495 0.051 Uiso 1 1 calc R . .
C16 C -0.3475(16) 0.1222(12) 0.8284(9) 0.034(4) Uani 1 1 d . . .
H16 H -0.3568 0.1781 0.8204 0.041 Uiso 1 1 calc R . .
C17 C -0.2713(15) 0.0977(10) 0.8827(8) 0.025(4) Uani 1 1 d . . .
H17 H -0.2294 0.1365 0.9102 0.031 Uiso 1 1 calc R . .
C18 C -0.2561(16) 0.0131(10) 0.8970(8) 0.025(2) Uani 1 1 d . . .
C19 C 0.0343(16) 0.1733(11) 0.9280(8) 0.027(3) Uani 1 1 d . . .
C20 C 0.2144(16) 0.0229(11) 0.9562(7) 0.027(3) Uani 1 1 d . . .
C21 C 0.0343(15) 0.0433(11) 0.8860(9) 0.029(4) Uani 1 1 d . . .
C22 C -0.1304(16) 0.1732(10) 1.0972(7) 0.024(4) Uani 1 1 d . . .
C23 C -0.2628(18) 0.1866(12) 1.2047(9) 0.038(5) Uani 1 1 d . . .
H23 H -0.2779 0.1305 1.2020 0.046 Uiso 1 1 calc R . .
C24 C -0.3156(18) 0.2294(13) 1.2586(8) 0.035(4) Uani 1 1 d . . .
H24 H -0.3641 0.2031 1.2929 0.042 Uiso 1 1 calc R . .
C25 C -0.296(2) 0.3116(14) 1.2612(9) 0.045(5) Uani 1 1 d . . .
H25 H -0.3335 0.3423 1.2970 0.054 Uiso 1 1 calc R . .
C26 C -0.2214(19) 0.3499(12) 1.2116(10) 0.041(5) Uani 1 1 d . . .
H26 H -0.2066 0.4059 1.2159 0.049 Uiso 1 1 calc R . .
C27 C -0.1671(16) 0.3075(9) 1.1549(8) 0.023(3) Uani 1 1 d . . .
H27 H -0.1202 0.3342 1.1202 0.028 Uiso 1 1 calc R . .
C28 C -0.1869(15) 0.2229(11) 1.1531(7) 0.022(4) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
W1 C19 1.953(17) . ?
W1 C21 1.957(17) . ?
W1 C20 1.990(16) . ?
W1 N1 2.161(14) . ?
W1 As1 2.6302(16) . ?
W1 I2 2.8303(13) . ?
W1 I1 2.8445(12) . ?
As1 C18 1.928(16) . ?
As1 C12 1.932(16) . ?
As1 C6 1.938(14) . ?
O1 C19 1.20(2) . ?
O2 C20 1.17(2) . ?
O3 C21 1.19(2) . ?
N1 C22 1.127(19) . ?
C1 C6 1.38(2) . ?
C1 C2 1.42(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.43(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.39(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(2) . ?
C5 H5 0.9300 . ?
C7 C12 1.38(2) . ?
C7 C8 1.46(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.35(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.32(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.44(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.39(2) . ?
C11 H11 0.9300 . ?
C13 C18 1.34(2) . ?
C13 C14 1.46(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.39(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.34(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.36(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.42(2) . ?
C17 H17 0.9300 . ?
C22 C28 1.46(2) . ?
C23 C24 1.35(2) . ?
C23 C28 1.39(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.36(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.37(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.40(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.40(2) . ?
C27 H27 0.9300 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C19 W1 C21 70.8(7) . . ?
C19 W1 C20 105.9(7) . . ?
C21 W1 C20 72.7(6) . . ?
C19 W1 N1 83.3(6) . . ?
C21 W1 N1 130.4(6) . . ?
C20 W1 N1 156.8(6) . . ?
C19 W1 As1 111.2(5) . . ?
C21 W1 As1 73.1(5) . . ?
C20 W1 As1 116.1(5) . . ?
N1 W1 As1 78.4(4) . . ?
C19 W1 I2 76.7(5) . . ?
C21 W1 I2 126.8(5) . . ?
C20 W1 I2 77.5(5) . . ?
N1 W1 I2 84.2(4) . . ?
As1 W1 I2 159.72(5) . . ?
C19 W1 I1 161.5(5) . . ?
C21 W1 I1 127.4(5) . . ?
C20 W1 I1 79.4(4) . . ?
N1 W1 I1 85.7(4) . . ?
As1 W1 I1 80.91(4) . . ?
I2 W1 I1 87.47(4) . . ?
C18 As1 C12 102.9(7) . . ?
C18 As1 C6 100.4(6) . . ?
C12 As1 C6 103.3(7) . . ?
C18 As1 W1 111.4(5) . . ?
C12 As1 W1 117.3(5) . . ?
C6 As1 W1 119.1(4) . . ?
C22 N1 W1 169.3(14) . . ?
C6 C1 C2 119.4(16) . . ?
C6 C1 H1 120.3 . . ?
C2 C1 H1 120.3 . . ?
C1 C2 C3 119.4(15) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C4 C3 C2 119.1(16) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 119.6(18) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 122.5(15) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C1 119.9(14) . . ?
C5 C6 As1 120.7(10) . . ?
C1 C6 As1 119.4(12) . . ?
C12 C7 C8 117.4(17) . . ?
C12 C7 H7 121.3 . . ?
C8 C7 H7 121.3 . . ?
C9 C8 C7 120.3(17) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C10 C9 C8 121.6(16) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 121.3(18) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C12 C11 C10 117.5(18) . . ?
C12 C11 H11 121.2 . . ?
C10 C11 H11 121.2 . . ?
C7 C12 C11 121.6(17) . . ?
C7 C12 As1 118.6(13) . . ?
C11 C12 As1 119.6(13) . . ?
C18 C13 C14 119.7(17) . . ?
C18 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 119.5(16) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C14 118.1(17) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 123.7(19) . . ?
C15 C16 H16 118.1 . . ?
C17 C16 H16 118.1 . . ?
C16 C17 C18 119.7(15) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C13 C18 C17 119.2(16) . . ?
C13 C18 As1 122.6(14) . . ?
C17 C18 As1 118.2(11) . . ?
O1 C19 W1 175.8(14) . . ?
O2 C20 W1 177.3(16) . . ?
O3 C21 W1 175.9(16) . . ?
N1 C22 C28 174.9(18) . . ?
C24 C23 C28 122.9(18) . . ?
C24 C23 H23 118.5 . . ?
C28 C23 H23 118.5 . . ?
C23 C24 C25 118.3(18) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
C24 C25 C26 120.8(18) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 122.1(18) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C28 C27 C26 116.5(16) . . ?
C28 C27 H27 121.7 . . ?
C26 C27 H27 121.7 . . ?
C23 C28 C27 119.3(15) . . ?
C23 C28 C22 120.3(16) . . ?
C27 C28 C22 120.4(15) . . ?
 
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.989
_refine_diff_density_max    2.737
_refine_diff_density_min   -0.987
_refine_diff_density_rms    0.212
